Materials Research.

2014; 17(4): 926-932

2014

DDOI: http://dx.doi.org/10.1590/1516-1439.253413

Rheological and Mechanical Characterization of

Poly (methyl methacrylate)/silica (PMMA/SiO2) Composites
Erik dos Santos Silvaa, Lourdes Aparecida Ribeiroa,b,
Maria Carolina Burgos Costa do Nascimentoc, Edson Noriyuki Itoc*
Graduate Program in Materials Science and Engineering, Federal University of Rio Grande do
NorteUFRN, Avenida Senador Salgado Filho, 3000, CEP 59078-970, Natal, RN, Brazil
b
Federal Institute of Bahia, Campus Simoes Filho, Simoes Filho, BA, Brazil
c
Department of Materials Engineering, Federal University of Rio Grande do NorteUFRN, Avenida
Senador Salgado Filho, 3000, CEP 59078-970, Natal, RN, Brazil
a

Received: November 19, 2013; Revised: June 9, 2014

The search for new materials with properties suitablefor specific applications has increased the
number of research studies to fill the market demands. The development of polymer composites by the
addition of inorganic fillers to the poly(methyl methacrylate) (PMMA) increases the potential use of
this polymer in various application fields. The main objective of this work was to study the rheological
and mechanical behavior of composites obtained from the addition of silica in two different types of
PMMA matrix: a common (PMMAc) and an elastomeric copolymer (PMMAel). The results showed
that the addition of silica particles to the PMMA matrix promoted an increase in torque, a decrease
in the melt flow index of composites and an increase in hardness compared to pure polymers. The
composites also showed a reduction of the maximum tensile strength for composites with PMMAc
matrix and maintenance of tensile strength for composites with PMMAel matrix. The average width
of scratch decreased due to a change in wear mechanism, attributed to the increase of hardness in the
composites obtained.
Keywords: polymer composites, poly (methyl methacrylate), silica, scratch, wear

1. Introduction
The development of materials science has brought
important contributions to the advancement of technology.
The constant search for new materials with optimized
performance and properties, for innovative applications
and improvement of existing materials, is a challenge, and
one of the reasons of technical and scientific development.
The use of composites as engineering materials is gaining
more space in various industry segments, since they provide
good synergy in the interaction between the different
components that form them, resulting in a range of properties
inherent to the material, and attributions (economical and
environmental) more interesting than their individual
components1,2. This properties of a composite material
depend not only upon the properties of the individual
component phases (matrix, filler, interphase), but also upon
their interaction3.
PMMA has high stiffness and excellent dimensional
stability, compared to other acrylic polymers widely used in
the production of transparent artifacts to replace glass4. The
incorporation of inorganic fillers into polymers can create
materials with higher mechanical strength, thermal stability
or with higher magnetic, optical or electrical properties.
The use of silica as filler leads to improved properties
such as increased rigidity, increased dimensional stability
*e-mail: ito@ufrnet.br

and reduced flammability5. The interaction at the interface

between them plays a crucial role in the properties and
performance of composites used in a particular application.
Ferreiraetal.6 studied the mechanical behavior of a
PMMA/SiO2 mixture for applications in sanitary and kitchen
equipment, varying the concentration of components and
particle size of the silica used. The results showed that the
material with higher silica content and finer grains exhibited
higher mechanical properties (maximum stress and Youngs
modulus), compared to material with lower silica content
and coarser grains. Fracture toughness was also evaluated,
being higher for the latter. Wangetal.7 evaluated the effect
of the interface on the thermal stability of PMMA/SiO2
hybrids by differential scanning calorimetry (DSC) and
thermogravimetry (TGA) techniques. The results showed
higher thermal stability for hybrids when compared to
PMMA.
Brostowetal.8 prepared nanocomposites of PMMA and
montmorillonite clay (MMT) in a co-rotational twin-screw
extrusion and injection molding, varying weight fraction
of MMT Brazilian clays. Dynamic friction and wear rate
of these composites were studied as a function of Brazilian
clay concentration.
Sugimotoetal.9 prepared reactive silica nanoparticles
and copolymerized them with methyl methacrylate. The
samples were analyzed by thermogravimetric analysis,

2014; 17(4)

Rheological and Mechanical Characterization of Poly (methyl methacrylate)/silica (PMMA/SiO2) Composites

dynamic mechanical analysis (DMA), Fourier transform

infrared spectroscopy (FTIR) and nuclear magnetic
resonance spectroscopy (NMR). Results showed that the
hybrids showed high transparency and increased Youngs
modulus, hardness and thermal stability.
Itoetal.10 studied the incorporation of silica obtained
from the controlled burning of Equisetum arvense L.
stem in two kinds of PMMA polymer matrix with and
without compatibilizer. The addition of these particles
promoted improvements in thermal stability and viscosity
of the composites produced. The mechanical properties
of composites; however, showed small changes when
compared to the pure polymer, probably due to the presence
of large agglomerates which might be negatively affecting
composites performance. The compatibilizer showed no
effectiveness interaction, and should not be used for low
silica concentrations.
Zou and Yoshida11 studied the effect of the size of silica
nanoparticles on the thermal decomposition of PMMA using
the thermogravimetric technique. The author considered
that the improvement of thermal stability depends on the
size, on the state of dispersion and on the surface area of
silica particles.
Avolioetal.12 synthesized PMMA nanocomposites with
silica nanoparticles modified by in situ polymerization. NMR
(nuclear magnetic resonance) experiments were performed to
evaluate the nature of interactions between organic and the
inorganic phases. The formation of an interphase consisting
of PMMA chains grafted onto the silica surface was observed.
The abrasion resistance and the glass transition temperature of
these materials were also evaluated. The abrasion resistance
of nanocomposites was improved due to changes in wear
mechanism. The increase in the glass transition temperature
was attributed to the strong interaction between polymer and
the modified silica particles.
Wear can be defined as a progressive loss of material
from the surface of a solid body due to mechanical action,
that is, the contact and relative movement of this body against
a solid, liquid or gaseous body13. Abrasive wear is related to
some mechanisms, including microcutting, microploughing
and microcracking (Figure1). Microploughing and
microcutting are dominant mechanisms in more ductile
materials and the occurrence of one of them depends on
the attack angle of abrasive particles. Microcutting occurs
from a critical attack angle, which is a function of the
material used and test conditions. The transition from
microploughing to microcutting also depends on the friction
coefficient. Microcracking is the wear mechanism most
characteristic in brittle materials.
The main aim of this work was to study the rheological
and mechanical properties of composites made with two types
of PMMA and silica obtained by mechanical mixing in single
screw extruder for new applications as engineering plastics.

and 1.1 g/10min (ASTM D 1238), respectively, acquired

from Unigel Plsticos S/A. The inorganic filler used was
precipitated silica particles (10SiO2.1H2O), TIXOSIL 333,
acquired from Rhodia.

2.2. Methodology
2.2.1. Particle
The laser diffraction particle size method was used for
determining the average particle size of silica. Ultrasound
was used before analysis to break up clumps for 10 minutes
in the presence of a deflocullant (Triton X -100) from
Aldrich. The equipment used was a Microtac, model S3500.

2.2.2. X-ray fluorescence (XRF)

Semi-quantitative analysis of powdered silica was
performed in a Shimadzu XRF -1800 equipment to provide
information about the chemical composition of this material.

2.2.3. Torque rheometry

Torque rheometry test was carried out in an internal
mixer (Rheomix 600) operating with roller-type rotors
coupled to a Haake-Bchler System 90 torque rheometer.
Rotation speed of 50 rpm and temperature of 220C were
used, with mixing time of 10 minutes. Polymers and
composites with 5 % silica were prepared directly in the
rheometer without previous extrusion. The weight was kept
constant at 50 g for all samples.

2.2.4. Sample preparation

Pure polymers and composites were processed on a
single-screw extruder model AX 16 from AX Plsticos
Mquinas Tcnicas LTDA with screw diameter D=16mm
and length/diameter ratio (L/D=26) and screw with
Maddock-type dispersive element. Before mixing, the
materials were previously dried in vacuum oven for 24 hours
at 60C. The temperature profile used during the extrusion
was 220/240/230C in the respective feeding/ mixing/matrix
zones with rotation of 40 rpm. Table1 shows the proportions
of materials prepared by extrusion.

2. Experimental
2.1. Materials
In this work, two types of PMMA (granules) were
used: a polymer Acrigel LEP100 (called PMMAc)
and an elastomeric copolymer Acrigel ECP800 (called
PMMAel) with melt flow indexes (230C/3.8 kg) of 3.8

927

Figure1. Wear mechanisms involved in abrasive wear13.

928

Silvaetal.

2.2.5. Injection molding

Specimens (ASTM D 638 Type I) were injection
molded in an Arburg machine model Allrounder 270S. The
processing conditions were: injection temperature profile
of 210/220/230/240/240C, mold temperature of 40C and
cooling time of 35 seconds.

Materials Research

According to Jillavenkatesaetal.17, knowing the size and

distribution of particles is a prerequisite for many processing
and manufacturing operations involving particulate
systems. Therefore, particle size has a significant effect on
the mechanical strength of composites, which generally
increases with smaller size of particles18-20.

2.2.6. Melt flow index (MFI)

3.1.3. Silica morphology

The melt flow index of unprocessed polymers and

processed materials was determined in a CEAST extrusion
plastometer, standardized according to ASTM D 1238 using
temperature of 230C and weight of 3.8 kilograms.

SEM analysis (Figure3) was performed not only to

characterize the morphology of precipitated silica but also
for carrying out measures related to particle size.
Figure3 shows that the particles do not have welldefined shape. The results of particle size characterization
and scanning electron microscopy indicate the need to
perform a processing step with higher shear rate in order to
achieve greater efficiency in silica dispersion. For particle
size measurement, the measurement of about 200 particles
was performed using image analysis software (Image J),
obtaining an average size of 11.52.7 m, approaching
the value obtained by laser diffraction.
Lau 21 showed that the mechanical properties of
composites and nanocomposites are affected by particle
size, particle type and in particular, by the particle/matrix
interfacial adhesion. Sumitaetal.22 reported the importance
of substituting microscale silica by particles in nanometric
scale, giving greater stiffness and resistance to polymers.

2.2.7. Tensile test

Tensile tests were performed in a universal Shimadzu
testing machine model AG-X 300 kN using type I specimen
of ASTM D 638. The test speed was 5 mm/min until
specimen rupture.

2.2.8. Scratch test

Scratch test was performed with a device made for this
task, based on the Hoffman scratch test equipment. The
equipment consists of a cart having a standard weight of
200g applied on the sliding surface with commercial steel
scriber brand Cortag. Three scratches were performed in
each sample, which were subsequently analyzed by light
microscopy in Olympus equipment, GX 51, and the average
widths (15 measurements for each scratch) were measured
with the aid of the Image J software. After assembly, the
entire apparatus had a weight of 214.7 g on the samples
assayed. The contact angle of the scriber of 85 was
measured using a Mitutoyo profile projector model PH- R14.

2.2.9. Hardness
The Rockwell M hardness measurements were
performed using a steel ball with diameter of inch,
pre-load of 10 kgf and load of 100 kgf on a Durometer brand
Pantec model RASN. Five measurements were performed
on each sample, in accordance with ASTM D 785.

3.2. Characterization of composites

3.2.1. Torque rheometry
In the processing of polymers, the rheological properties
depend on operating (temperature, pressure, flow, etc.) and
Table1. Materials processed by extrusion.
Materials

% Weight fraction

PMMAc/SiO2
PMMAel/SiO2

100
99.5/0.5
99/1
95/5

3. Results and Discussion

3.1. Silica characterization
3.1.1. Silica FRX
The X-ray fluorescence analysis (Table2) aimed to
provide quantitative information on the composition of
precipitated silica used in this work.
The results show the chemical composition of
compounds present in the test material containing silica
in greater amounts and compounds such as sulfur trioxide
and copper oxide in smaller amounts, probably from the
inefficient filtration and washing process carried out in
the industry to remove all traces of chemical salts and byproducts of the precipitation process.

Table2. FRX of precipitated slica.

Content

(%)

SiO2
SO3
CuO

96.73
2.93
0.34

3.1.2. Laser diffraction

Figure2 shows the accumulated and discrete particle
size distribution curve of the silica used. The analysis
showed that the measures ranged from 2.7 to 74 m, with
a mean diameter of 13.4 m.

Figure2. Silica particle size characterization.

2014; 17(4)

Rheological and Mechanical Characterization of Poly (methyl methacrylate)/silica (PMMA/SiO2) Composites

929

Figure3. SEM images of silica with magnification of: a) 1000x; b ) 1500x.

structural parameters (molecular weight, molecular weight

distribution, etc.). Thus, it is recommended to measure
rheological properties such as viscosity under conditions
closer or similar to processing conditions23. The torque
rheometer results are shown as a torque versus time curve
for polymers and for composites with 5 % silica without
prior extrusion, as can be seen in Figure4.
Torque peak at the beginning of processing is called
the load peak, which refers to the torque required to
maintain rotation speed programmed in the rheometer,
while the material is flowing into the camera. Initially,
PMMA polymer samples were tested to identify the
polymer behavior in relation to the processing conditions.
It was found that much of the mass added to the equipment
was melted 2 minutes after processing began. It was also
observed that the PMMAc/SiO2 (95/5) curve is shifted to
the right due to a delay in the supply of this sample into
the rheometer.
The results showed that although PMMAel has higher
torque after 10 minutes when compared to PMMAc, the
increase in torque promoted by SiO2 addition was minimized
for PMMAel, indicating that much of the silica may have
been attracted by the rubber phase of copolymer, thus
reducing the effect of interaction of PMMA with silica
particles. After 10 minutes of mixing, the increase in torque
promoted by the addition of silica particles into the PMMAc
matrix was about 20%. According to Marconcinietal.24,
the increased torque during test is indicative of increased
viscosity of the composite compared to the pure polymer,
showing an interaction between the system components,
similar to those presented in this work, except that the
sample used the compatibilizer. Clearly, the rheological
evidences presented are not sufficient to prove the nature of
the interactions between the copolymer and silica, requiring
complementary investigative techniques.

3.2.2. Melt flow index measurements

The melt flow index (MFI) of processed unprocessed
polymers is shown in Figure5.

Figure4 . Torque rheometry of polymers and composites with 5

% silica.

These results show a reduction in the melt flow index

of composites in both matrices with increasing silica
concentration, since the addition of fillers increases the
viscosity. The melt flow index is an empirically defined
parameter, inversely proportional to the viscosity of the
material at specific temperature and shear rate25. Unlike
PMMAc, PMMAel has rubber particles present as dispersed
phase in its matrix, which contributed to a lower melt flow
index (higher viscosity). In MFI, the flow to pass through
the die is elongational and needs to direct the molecules in
the flow direction. This directing is hindered in the presence
of the silica particles, and even more in the presence of
elastomeric phase, providing a higher decrease in MFI for
composites with PMMAel. Results also indicate that there
was a slight increase in the melt flow index of polymers after
processing, indicating the occurrence a small degradation
of these materials during this step. MFI results should be
cautiously interpreted due to the fact that the method of
analysis may present several flaws as the results are very
sensitive to measurement procedure details, especially for
low MFI polymers. It should also be mentioned that MFI
values are not truly useful to predict the actual processing
conditions, since many commercial thermoplastic are

930

Silvaetal.

Materials Research

pseudoplastics or have decreased viscosity with increasing

shear rate, being usually processed at much higher rates than
those imposed during the measurement of this property26.

3.2.3. Tensile test

Figure5. Graph comparing the melt flow index of polymers and

processed composites.
Table3. Tensile strength results of polymers and composites.
Composition (% mass)
PMMAc (100)
PMMAc/SiO2 (99.5/0.5)
PMMAc/SiO2 (99/1)
PMMAc/SiO2 (95/5)
PMMAel (100)
PMMAel/SiO2 (99.5/0.5)
PMMAel/SiO2 (99/1)
PMMAel/SiO2 (95/5)

Maximum tensile strength

(MPa)
64.20.6
57.72.3
55.21.6
37.92.6
32.90.8
34.20.2
34.20.1
34.60.3

The maximum tensile strength of pure polymers and of

composites obtained at concentrations of 0.5, 1 and 5% by
weight was determined through tensile tests by evaluating
the effect of silica concentration on this property. Table3
presents the average maximum tensile strength values of
injection molded samples.
The mechanical properties of composites suffered some
variations in relation to pure polymers. This tableshows
a significant decrease in the tensile strength for PMMAc/
SiO2 composites with increasing silica concentration. This
reduction may be related to the presence of silica particles
of irregular shape, which can act as stress concentrators, thus
weakening the material. For PMMAel/SiO2 composites, the
addition of silica particles not provide any change in tensile
strength of these materials, probably indicating that the
interaction of the particles with this type of matrix should
have been decreased due to interactions with the rubber
phase of the copolymer. These results were also observed by
Marconcinietal.24, who used silica particles obtained from
the controlled burning of Equisetum arvense L. stem using
conditions similar to those described by DeSouzaetal.27.
Figure6 shows comparative stress versus deformation
curves of a representative sample of polymers and their
composites, constructed with maximum tensile strength
values that came closest to the average. The deformation
values presented for comparative purposes were determined
from the displacement of the machines movable head.
Based on the curves shown, no significant change with
respect to stiffness was observed for both PMMAc and
PMMAel matrices. For PMMAc and their composites the
value of Youngs modulus was approximatelly 2.5 GPa
and to PMMAel and their composites was 1.4 GPa. Thus,
there is evidence that the amount of reinforcement may
not have directly influenced this property, which is most
strongly affected by the type of reinforcement than by the
added content18.

Figure6. Comparative stress versus deformation curves: a) PMMAc matrix; b) PMMAel matrix.

2014; 17(4)

Rheological and Mechanical Characterization of Poly (methyl methacrylate)/silica (PMMA/SiO2) Composites

With respect to the elongation at rupture observed in the

graphs of Figure6, there is a reduction due to the increase
in the silica concentration for all composites studied, being
more significant for PMMAel/SiO2, reducing about 3 times
its deformation. This behavior can be explained by the fact
that silica particles have different geometries, and may act as
stress concentrators, which can be seen in the micrographs
shown in Figure3.

3.2.4. Rockwell M hardness

The hardness test results are shown in Table4.
With respect to surface hardness, the results show that
the silica particles were effective in increasing this property
to PMMAc, about 20% to PMMAc/SiO2 (95/5) composite,
while for PMMAel no significant variation was observed.
Although there is evidence that the particles are attracted
into the copolymer elastomeric phase, the amount of filler
Table4. Hardness results the samples obtained by injection
molding.
Injected specimens

Rockwell Hardness (HRM)

PMMAc (100)
PMMAc/SiO2 (99.5/0.5)
PMMAc/SiO2 (99/1)
PMMAc/SiO2 (95/5)
PMMAel (100)
PMMAel/SiO2 (99.5/0.5)
PMMAel/SiO2 (99/1)
PMMAel/SiO2 (95/5)

68.00.7
71.00.7
76.21.9
80.20.8
40.42.7
41.62.1
44.61.5
45.21.3

Table5. Average width of scratch.

PMMA/SiO2
(% mass)
(100/0)
(99,5/0,5)
(99/1)
(95/5)

Width of scratch (m)

PMMAc/SiO2

PMMAel/SiO2

129.79.0
122.510.1
118.53.9
137.65.7

197. 410.6
168.812.0
164.76.1
158.612.9

Figure7. Optical microscopy images of scratch.

931

and dispersion of these particles may not be sufficient to

promote better hardness results.

3.2.5. Scratch assay

The average width of scratch is shown in Table5.
These results show a decrease in the average scratch
width with increasing silica concentration, except for
PMMAc/SiO2 (95/5), which showed an increase in the
average width of the tear, which may have been caused by the
pullout of part of the polymer with the silica during scratch,
which is typical of the microcracking wear mechanism.
A visual difference was also observed between scratch
produced in each polymer and composite studied, as
illustrated in Figure7.
Figure 7 shows the transition from microploughing to
microcutting wear mechanisms in composites with PMMAel
matrix with increased silica concentration. Normally, the
mechanism shifts from microploughing to microcutting
with increasing hardness of the material, and even greater
increases in hardness result in shift from microcutting to
microcracking13. Composite with PMMAc matrix only
show the microcutting wear mechanism, typical of brittle
materials of high hardness.

4. Conclusions
The effects of adding silica particles to two types of
PMMA matrices were evaluated in terms of the mechanical
and rheological properties of these materials. With respect
to the tensile mechanical properties, it was observed that
there was a reduction in tensile strength for composites
with PMMAc matrix and a maintenance of this property
for composites with PMMAel matrix as a function of
increasing silica concentration. There was a significant
increase in hardness for both types of PMMA matrices,
being more significant for polymer with PMMAc matrix,
changing the wear mechanism of composites studied. The
torque rheometry and melt flow index results showed that
increasing the silica concentration in the PMMA matrices
resulted in general increase in the system viscosity and
hence in a decrease in the melt flow index. The incorporation
of silica particles into the PMMA matrix is feasible and
promising to obtain composites with thermoplastic matrix.

932

Silvaetal.

Acknowledgements
To CNPq for the fellowship granted. To FINEP
agreement 01.10.0697.00 for infrastructure support. To
Unigel Plsticos S/A and Rhodia for the kind donation of

Materials Research

materials. To Professor Jos Marconcini from EMBRAPA

Instrumentao-So Carlos for the injection of test
specimens and to the Group of Studies in Tribology-UFRN
for the use of the hardness equipment.

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